CN104152147A - Rare earth oxysalt phosphor and its application - Google Patents

Rare earth oxysalt phosphor and its application Download PDF

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CN104152147A
CN104152147A CN201410406093.8A CN201410406093A CN104152147A CN 104152147 A CN104152147 A CN 104152147A CN 201410406093 A CN201410406093 A CN 201410406093A CN 104152147 A CN104152147 A CN 104152147A
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fluor
oxysalt
rare earth
light
twinkler
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CN104152147B (en
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王海容
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Abstract

The invention relates to a rare earth oxysalt phosphor and its application. The chemical composition of the phosphor is (RE1-xLnx)yMzRr(A1-aDa)bOcEd, wherein RE contains at least one of Sc, Y, La, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and Bi; Ln contains at least one of Ce and Pr; M contains at least one of Li, Na, K, Rb and Cs; R contains at least one of Ca, Sr, Ba, Mg, Zn, Cd, Ni, Mn, Zr, Hf and Ti, and at least contains Zr; A contains at least one of Al, B, Ga and Cr; D contains at least one of P, V, Nb and Ta; E contains at least one of F and Cl; O is oxygen; and x is more than 0 and not more than 0.5, y is not less than 0.5 and less than 3, z is not less than 1 and not more than 4, r is not less than 0 and not more than 4, a is not less than 0 and less than 0.5, b is not less than 3 and not more than 5, c is more than 6 and not more than 16, d is not less than 0 and not more than 2, and the value of a*b is less than z. The phosphor has excellent luminescence and temperature quenching characteristics.

Description

A kind of rare earth oxysalt fluor and application thereof
Technical field
The present invention relates to solid luminescent material field, relate in particular to a kind of rare earth oxysalt fluor, also relate to the luminous element and the pigment that contain this fluor.
Background technology
Fluor is applied to illumination and the every field showing, especially along with the development of semiconductor lighting technology, the fluor being applied in white light LEDs has been subject to paying close attention to more and more widely.White light LEDs photoelectric transformation efficiency is high, energy-conserving and environment-protective, long service life, safe and reliable, is acknowledged as green illumination light source of future generation.The current white light LEDs of realizing mainly contains 3 kinds of approach, the first is to be combined to form white light by red, green and blue look LED chip, but it is more difficult to realize by this method white light, because will consider the drive characteristic of three different colours chips, very complicated in circuit layout.The second is to use quantum effect, uses the same semi-conductor of different-grain diameter size to prepare LED chip to realize white light, and the white light LEDs that this method realizes has higher efficiency, but cost is higher, simultaneously technical also immature.The third is to add that with the LED chip of sending out UV-light or blue light fluor realizes white light, and this method is the most simple, is also the most ripe method simultaneously.
LED has been subject to showing great attention to of countries in the world as the green illumination light source of energy-conserving and environment-protective of new generation, utilize ultraviolet or blue-ray LED excited fluophor and produce the main flow that white light is current white light LEDs development, the performance of fluor directly affects brightness, colour temperature, thermostability and the color developing etc. of white light LEDs.Along with white light LEDs is to the development of high-power direction, the working temperature of LED is more and more higher, and the working temperature of current great power LED chips can reach 180 DEG C, and this fluor that just requires to be applied in white light LEDs must possess excellent temperature quenching characteristic.
The fluor using in white light LEDs is at present mainly blue-light excited YAG:Ce bloom, and it can effectively absorb near blue light 460nm, excited by it and launches gold-tinted, and produce white light with LED blue light.But owing to lacking red and green spectral composition in the emmission spectrum of YAG:Ce bloom, the white light LEDs colour rendering index made from it is low, can not truly show the color of object; Simultaneously the temperature quenching characteristic of YAG:Ce bloom is not outstanding, when its luminous intensity is room temperature in the time of 150 DEG C, drops to 74% 87%, 200 DEG C of luminous intensity time, can not meet the application demand of large power white light LED.
The LuAG fluor that LED newly developed mainly contains silicate phosphor, nitride and oxynitride fluor and improves on YAG basis with fluor in recent years.Silicate phosphor has wider adjustable emission wavelength, and luminous efficiency is also higher, but existing silicate phosphor temperature profile is poor, as Sr 3siO 5: Eu 2and Sr 2siO 4: Eu 2luminance factor room temperature at 150 DEG C declines respectively 32% and 62%, thereby the practical application of current silicate phosphor few.
Nitride and oxynitride fluor be because having wider excitation spectrum and emmission spectrum, and heatproof characteristic and chemical stability be all better than YAG bloom, received the very big concern of white light LEDs industry.With regard to current nitride and oxynitride fluor, fluor that can be practical is mainly Sr 2si 5n 8: Eu rouge and powder and CaAlSiN 3: Eu rouge and powder.Sr 2si 5n 8: the luminosity of Eu rouge and powder is higher, but because self physical and chemical stability is with respect to CaAlSiN 3: Eu rouge and powder is slightly poor, and its luminosity at 150 DEG C is 74% while being 86%, 200 DEG C under room temperature, has limited to a certain extent it and has applied on a large scale.CaAlSiN 3: Eu rouge and powder has good physical and chemical stability and temperature quenching characteristic, and its luminosity at 150 DEG C is 82% while being 90%, 200 DEG C under room temperature, but its transmitting main peak is 650nm, in dark red wave band, luminosity deficiency, awaits further raising.
Improved LuAG:Ce fluor on the basis of YAG:Ce bloom, there is good luminous efficiency and excellent temperature quenching characteristic, its luminous efficiency under blue-ray LED excites is about 90%, luminosity at 150 DEG C is 97% under room temperature, 200 DEG C time, be 90%, but the LuAG:Ce fluor prices of raw and semifnished materials are more expensive, and synthesis technique is comparatively complicated.
In sum, the aspect such as luminous efficiency and temperature cancellation characteristic of the fluor using at present under ultraviolet LED or blue-ray LED excite can't meet the needs of practical application completely, and therefore the efficient LED of development of new becomes the focus of domestic and international research with fluor.
Summary of the invention
The object of the invention is for the problems referred to above, the fluor that a kind of physical and chemical stability is good is provided, it has higher luminous efficiency than existing all kinds of fluor, more excellent temperature cancellation characteristic.
Another object of the present invention is to use this fluor to provide that luminous efficiency is high, the luminous element of Heat stability is good.
Another object of the present invention is to provide the pigment that has used this fluor.
In order to solve above-mentioned problem, the present inventor conducts in-depth research the various oxysalt fluor taking Ce as main activator, found that, the rare earth oxysalt fluor that contains specific chemical constitution is the excellent fluor that solves above-mentioned problem, thereby has realized the present invention.
The object of the invention is to be achieved through the following technical solutions:
The 1st invention is a kind of rare earth oxysalt fluor, it is characterized in that: chemical constitution general formula is: (RE 1-xln x) ym zr r(A 1-ad a) bo ce d, wherein, RE is at least one in Sc, Y, La, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Bi; Ln is at least one in Ce, Pr; M is at least one in Li, Na, K, Rb, Cs; R be in Ca, Sr, Ba, Mg, Zn, Cd, Ni, Mn, Zr, Hf, Ti at least one and at least contain Zr; A is at least one in Al, B, Ga, Cr; D is at least one in P, V, Nb, Ta; E is at least one in F, Cl; O is oxygen; 0 < x < 0.5,0.5≤y < 3,1≤z≤4,0≤r≤4,0≤a <, 0.5,3≤b≤5,6 < c≤16,0≤d≤2, a × b < z.
The 2nd invention is the related rare earth oxysalt fluor of the 1st invention, it is characterized in that: 0 < x < 0.5,1≤y≤2,1.5≤z≤2.5,0≤r≤3,0≤a < 0.5,3.5≤b≤4.5,9≤c≤14,0≤d≤1, a × b < z.
The 3rd invention is that 1st～2 any one are invented related rare earth oxysalt fluor, it is characterized in that: 0 < x < 0.5, y=2, z=2, r=0,0≤a < 0.5, b=4,10≤c < 12, d=0, a × b < z.
The 4th invention is a kind of rare earth oxysalt fluor, it is characterized in that: chemical constitution general formula is: (RE 1-xln x) yr p(A 1-qd q) mo ce d, wherein, RE is at least one in Sc, Y, La, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Bi; Ln is at least one in Ce, Pr; R be in Ca, Sr, Ba, Mg, Zn, Cd, Ni, Mn, Zr, Hf, Ti at least one and at least contain Zr; A is at least one in Al, B, Ga, Cr; D is at least one in P, V, Nb, Ta; E is at least one in F, Cl; O is oxygen; 0 < x < 0.5,0.5≤y < 3,3≤p≤5,0≤q <, 0.5,1 < m≤4,6 < c≤16,0≤d≤2.
The 5th invention is the related rare earth oxysalt fluor of the 4th invention, it is characterized in that: 0 < x < 0.5,1≤y≤2, p=4,0≤q <, 0.5,2≤m≤3,11≤c≤12,0≤d≤1.
The 6th invention is that 4th～5 any one are invented related rare earth oxysalt fluor, it is characterized in that: 0 < x < 0.5, y=1, p=4,0≤q < 0.5, m=3, c=12, d=0.
The 7th invention is that 4th～5 any one are invented related rare earth oxysalt fluor, it is characterized in that: 0 < x < 0.5, y=2, p=4,0≤q < 0.5, m=2, c=12, d=0.
The 8th invention is a kind of luminous element, it comprises the 1st twinkler and the 2nd twinkler, the 1st twinkler sends the light with the 1st luminescent spectrum, the 2nd twinkler has at least a portion of the light of the 1st luminescent spectrum described in absorbing, and sends the light with 2nd luminescent spectrum different with described the 1st luminescent spectrum; It is characterized in that: contain the described rare earth oxysalt fluor of 1st～7 any one invention as the 2nd twinkler.
The 9th invention is the related luminous element of the 8th invention, it is characterized in that: especially use photodiode or laser diode as the 1st twinkler, or discharge lamp based on low pressure or high pressure, or electroluminescent lamp.
The 10th invention is a kind of pigment, it is characterized in that: contain the described rare earth oxysalt fluor of 1st～7 any one invention.
The rare earth oxysalt fluor of the present invention use that can also be associated with other ultraviolet source or for example blue light OLED of blue light source, or be combined with blue light EL luminescent material.EL represents electroluminescent.
Brief description of the drawings
Fig. 1 is the excitation spectrum of the embodiment of the present invention 1 fluor and the 460nm wavelength utilizing emitted light spectrogram under blue-light excited.
Fig. 2 is the temperature quenching performance diagram of the commercial fluor of the embodiment of the present invention 1 fluor and comparative example YAG under 460nm wavelength is blue-light excited.
Embodiment
Rare earth oxysalt fluor of the present invention can adopt the technique preparations such as high temperature solid phase synthesis, coprecipitation method, sol-gel method, microwave sintering synthesis method, the technological process of its high temperature solid phase synthesis is: the simple substance or the compound that take respective element according to chemical formula component, and add boric acid, halogenide, alkaline carbonate at least one as fusing assistant, the addition of fusing assistant is 0.01～10% of raw material total mass.After ground and mixed is even, in reducing atmosphere, at 800 DEG C～1800 DEG C, sintering obtains product for 1～30 hour.In addition, in order to obtain the uniform fluor of crystalline phase, also the fluor obtaining can be repeated to pulverize, fire again.Described reducing atmosphere is at least one in charcoal, carbon monoxide, hydrogen, nitrogen, ammonia.
Below by embodiment, the present invention is described more specifically, but only otherwise exceed aim of the present invention, the present invention is not subject to any restriction of following embodiment.
Embodiment 1:Li 2y 1.86al 3b 0.1p 0.9o 10.9: Ce 0.14synthesizing of fluor:
At chemical constitution general formula (RE 1-xln x) ym zr r(A 1-ad a) bo ce din, set RE=Y, Ln=Ce, M=Li, A=(Al, B), D=P, weighing various raw materials, is Li: Y: Al: B: P: O: Ce=2 so that form the mol ratio of ion: 1.86: 3: 0.1: 0.9: 10.9: 0.14 (x=0.07, y=2, z=2, r=0, a=0.225, b=4, c=10.9, d=0).
Take 0.75gLi 2cO 3, 2.08gY 2o 3, 1.53gAl 2o 3, 0.06gH 3bO 3, 1.19g (NH 4) 2hPO 4, 0.24gCeO 2, after abundant ground and mixed is even, pack alumina crucible roasting in reducing atmosphere into, in 1560 DEG C of insulations 2 hours, obtain described fluor.Its excitation spectrum and emmission spectrum are shown in Fig. 1, and emmission spectrum halfwidth is about 112nm, and emmission spectrum main peak is in the green glow region of 540nm; Excitation spectrum is a bimodal excitation spectrum in broadband, and two bands of a spectrum that are positioned at 342nm and 455nm place by peak value form, and main excitation peak is positioned at 455nm place, can be good at mating with the emmission spectrum of blue-ray LED; Its luminous intensity is in table 1, the fluor that the present invention makes as can be seen from Table 1, and under 460nm wavelength blue-light excited, the luminous intensity of luminous intensity when its room temperature and 200 DEG C is all higher than the commercial fluor of comparative example YAG.
Fig. 2 is embodiment 1 Li 2y 1.86al 3b 0.1p 0.9o 10.9: Ce 0.14the temperature quenching performance diagram of the commercial fluor of fluor and comparative example YAG under 460nm wavelength is blue-light excited.Embodiment 1 fluor has excellent temperature quenching characteristic as can be seen from Figure 2, and the luminous intensity at 150 DEG C is 84% while being 92%, 200 DEG C under room temperature.
Embodiment 2～20:
At chemical constitution general formula (RE 1-xln x) ym zr r(A 1-ad a) bo ce din, set RE=(Y, Lu, Gd, La, Tb, Sm), Ln=(Ce, Pr), M=(Li, K), R=(Sr, Zr), A=(Al, B, Ga), D=P, E=Cl, the chemical formula composition concrete by each embodiment in table 1 takes various raw materials, and preparation process is identical with embodiment 1, and the characteristics of luminescence of the fluor obtaining is in table 1.
The chemical formula of table 1 embodiment 1～20 and the characteristics of luminescence thereof (excitation wavelength is 460nm)
Can be found out by table one, in table one, listed fluor is under 460nm is blue-light excited, emmission spectrum scope has contained the green glow of 525nm～611nm to ruddiness region, and the luminescent properties of most fluor is all better than commercial YAG, because of but the blue-ray LED fluor of a class excellent performance.
Embodiment 21:Y 0.94srCaZr 2al 2.9b 0.1o 12: Ce 0.06synthesizing of fluor:
At chemical constitution general formula (RE 1-xln x) yr p(A 1-qd q) mo ce din, set RE=Y, Ln=Ce, R=(Sr, Ca, Zr), A=(Al, B), weighing various raw materials, is Y: Sr: Ca: Zr: Al: B: O: Ce=0.94 so that form the mol ratio of ion: 1: 1: 2: 2.9: 0.1: 12: 0.06 (x=0.06, y=1, p=4, q=0, m=3, c=12, d=0).
Take 2.10gY 2o 3, 1.476gSrCO 3, 1.0gCaCO 3, 2.46gZrO 2, 1.48gAl 2o 3, 0.06gH 3bO 3, 0.1gCeO 2, after abundant ground and mixed is even, pack alumina crucible roasting in reducing atmosphere into, in 1420 DEG C of insulations 2 hours, obtain described fluor.Its emmission spectrum halfwidth is about 120nm, and emmission spectrum main peak is in the blue green light region of 497nm; Excitation spectrum is the continuous wide band excitation spectrum within the scope of 320nm～430nm, excites main peak to be positioned at 415nm place, can be good at mating with the emmission spectrum of near-ultraviolet light LED; Under the near ultraviolet excitation of 400nm wavelength, luminous intensity when its room temperature is Sr 4al 14o 25: the luminous intensity of 132%, 200 DEG C of Eu light-emitting phosphor intensity is Sr 4al 14o 25: 145% of Eu light-emitting phosphor intensity, because of but a kind of near-ultraviolet light LED fluor of excellent performance.
Embodiment 22～31:
At chemical constitution general formula (RE 1-xln x) yr p(A 1-qd q) mo ce din, set RE=(Y, Lu), Ln=Ce, R=(Sr, Ca, Mg, Zr), A=(Al, B, Ga), D=P, E=F, the chemical formula composition concrete by each embodiment in table 2 takes various raw materials, and preparation process is identical with embodiment 21, and the characteristics of luminescence of the fluor obtaining is in table 2.
The chemical formula of table 2 embodiment 21～31 and the characteristics of luminescence thereof (excitation wavelength is 400nm)
Can be found out by table two, in table two, listed fluor is under 400nm near ultraviolet excitation, and emmission spectrum scope has contained blue light and the blue green light region of 445nm～512nm, because of but a class is applicable to the fluor of near-ultraviolet light LED.
Fluor of the present invention shows than luminous, the more excellent thermal stability of the higher briliancy of existing fluor, so it is suitable for white light emitting device, lighting fixtures, VFD, FED, PDP, CRT etc.In addition, fluor of the present invention can easily be adjusted emission wavelength, so practicality is industrially large, can expect that from now on flexible Application is in the design of material of various light-emitting devices, illumination, image display device, the development of Promoting Industrial.
Although utilize specific mode to understand in detail the present invention, it will be apparent to those skilled in the art that and can carry out multiple change in the intent and scope of the present invention not departing from.

Claims (10)

1. a rare earth oxysalt fluor, is characterized in that: the chemical constitution general formula of described fluor is:
(RE 1-xln x) ym zr r(A 1-ad a) bo ce d, wherein, RE is at least one in Sc, Y, La, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Bi; Ln is at least one in Ce, Pr; M is at least one in Li, Na, K, Rb, Cs; R be in Ca, Sr, Ba, Mg, Zn, Cd, Ni, Mn, Zr, Hf, Ti at least one and at least contain Zr; A is at least one in Al, B, Ga, Cr; D is at least one in P, V, Nb, Ta; E is at least one in F, Cl; O is oxygen; 0 < x < 0.5,0.5≤y < 3,1≤z≤4,0≤r≤4,0≤a <, 0.5,3≤b≤5,6 < c≤16,0≤d≤2, a × b < z.
2. rare earth oxysalt fluor according to claim 1, it is characterized in that: 0 < x < 0.5,1≤y≤2,1.5≤z≤2.5,0≤r≤3,0≤a < 0.5,3.5≤b≤4.5,9≤c≤14,0≤d≤1, a × b < z.
3. according to the rare earth oxysalt fluor described in claim 1～2 any one, it is characterized in that: 0 < x < 0.5, y=2, z=2, r=0,0≤a < 0.5, b=4,10≤c < 12, d=0, a × b < z.
4. a rare earth oxysalt fluor, is characterized in that: the chemical constitution general formula of described fluor is:
(RE 1-xln x) yr p(A 1-qd q) mo ce d, wherein, RE is at least one in Sc, Y, La, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Bi; Ln is at least one in Ce, Pr; R be in Ca, Sr, Ba, Mg, Zn, Cd, Ni, Mn, Zr, Hf, Ti at least one and at least contain Zr; A is at least one in Al, B, Ga, Cr; D is at least one in P, V, Nb, Ta; E is at least one in F, Cl; O is oxygen; 0 < x < 0.5,0.5≤y < 3,3≤p≤5,0≤q <, 0.5,1 < m≤4,6 < c≤16,0≤d≤2.
5. rare earth oxysalt fluor according to claim 4, is characterized in that: 0 < x < 0.5,1≤y≤2, p=4,0≤q <, 0.5,2≤m≤3,11≤c≤12,0≤d≤1.
6. according to the rare earth oxysalt fluor described in claim 4～5 any one, it is characterized in that: 0 < x < 0.5, y=1, p=4,0≤q < 0.5, m=3, c=12, d=0.
7. according to the rare earth oxysalt fluor described in claim 4～5 any one, it is characterized in that: 0 < x < 0.5, y=2, p=4,0≤q < 0.5, m=2, c=12, d=0.
8. a luminous element, it comprises the 1st twinkler and the 2nd twinkler, the 1st twinkler sends the light with the 1st luminescent spectrum, has at least a portion of the light of the 1st luminescent spectrum, and send the light with 2nd luminescent spectrum different with described the 1st luminescent spectrum described in the 2nd twinkler absorbs; It is characterized in that: as the 2nd twinkler containing the rare earth oxysalt fluor described in good grounds claim 1～7 any one.
9. luminous element according to claim 8, is characterized in that: use photodiode or laser diode as the 1st twinkler, or discharge lamp based on low pressure or high pressure, or electroluminescent lamp.
10. a pigment, is characterized in that: described pigment is containing the rare earth oxysalt fluor described in good grounds claim 1～7 any one.
CN201410406093.8A 2014-08-15 2014-08-15 A kind of rare earth oxysalt fluorophor and application thereof Active CN104152147B (en)

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